CN101914059B - Analytical reagent for detecting trace lead as well as preparation method and application thereof - Google Patents
Analytical reagent for detecting trace lead as well as preparation method and application thereof Download PDFInfo
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- CN101914059B CN101914059B CN 201010256395 CN201010256395A CN101914059B CN 101914059 B CN101914059 B CN 101914059B CN 201010256395 CN201010256395 CN 201010256395 CN 201010256395 A CN201010256395 A CN 201010256395A CN 101914059 B CN101914059 B CN 101914059B
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- analytical reagent
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Abstract
The invention discloses a new analytical reagent for detecting trace lead, which has the chemical structure represented by the general formula (I). The analytical reagent is synthesized by the following two steps of reaction: firstly, using sulfanilic acid to prepare diazonium salt; then, coupling with 8-azly quinaldine to obtain the analytical reagent. The invention provides a new method for detecting trace lead based on the newly synthesized analytical reagent, and the method is applied to analysis tests in the tobacco industry. The defect of relatively low sensitivity of absorption photometry is overcome, so that the common photometry can be used for detecting mug/g level lead. The detection results of the method are consistent with the results of the graphite furnace atomic absorption method.
Description
Technical field
The present invention relates to the analytical chemistry field, more particularly, the present invention relates to a kind of analytical reagent that lead in tobacco and the additive thereof is measured.Simultaneously, the invention still further relates to the preparation method of this reagent and the application in tobacco industry.
Background technology
Lead in the tobacco is a kind of harmful element, and mensuration plumbous in tobacco, cigarette supplementary and the cigarette additive is significant to guaranteeing the cigarette product security.In the prior art, the method for measuring of lead content has spectrophotometry, atomic absorption method, atomic fluorescence method, plasma emission spectroscopy method, Waters Using ICP-MS etc.Spectrophotometry is simple because of plant and instrument, cost is low, is the most frequently used method.
The GB of China adopts the dithizone-extraction light-intensity method at present, and this method need be used chloroform extraction, and not only troublesome poeration, and consumption of organic solvent is big, easy contaminate environment, and it is also many to introduce error component.Though the plumbous report of other spectrphotometric method for measuring was arranged in recent years, because lead content is very low in the sample, need could accurately measure with light-intensity method after the enrichment, can not adapt to and produce actual needs, need improve urgently.
Summary of the invention
The objective of the invention is to deficiency, a kind of new analytical reagent is provided to prior art.
Another object of the present invention provides a kind of preparation method of said analytical reagent.
Further aim of the present invention provides the application of said analytical reagent in measuring trace lead.
The object of the invention is achieved through following technical proposals.
* except as otherwise noted, the percentage ratio that is adopted among the present invention is mass percent.
A. the present invention has carried a kind of new analytical reagent, and it has following structural formula:
Its called after 5-p-sulfonic acid base benzeneazo-8-amidoquinaldine.
B. the invention provides a kind of preparation method of said analytical reagent, this method adopts following step:
(1) Sulphanilic Acid with 0.02mol is dissolved in the 400ml absolute ethyl alcohol, adds the 2g sodium amide, and heating in water bath refluxed 4 hours;
(2) add the 8g Isopentyl nitrite, refluxed 30 minutes again, cooling makes diazonium salt;
(3) the 8 amino 8-amidoquinaldines of adding 0.02mol in diazonium salt solution, 2.5g yellow soda ash stirred 0.5 hour, placed liquid, and the most ethanol of pressure reducing and steaming leaches deposition and can get bullion;
(4) bullion is promptly obtained required analytical reagent 2～3 times with ethyl alcohol recrystallization.
C. the present invention is based on new synthetic analytical reagent, the novel method of measuring trace lead be provided, and this method is applied in the analytical test of tobacco industry:
(1) accurately takes by weighing sample (tobacco, cigarette supplementary or cigarette additive) 0.2g in tetrafluoroethylene microwave digestion jar, add 1.5mL concentrated nitric acid and 2mL 30%H
2O
2, in the microwave digestion stove, digest 10min; Digested back heating evaporation on hot plate and done,, changed in the 50mL tube comparison tubes with the dissolving with hydrochloric acid residue of 20mL 5% near; Add 5-p-sulfonic acid base benzeneazo-8-amidoquinaldine solution 4mL of 0.1% then, fully shake up, place 10min, colour developing liquid with the flow velocity of 10mL/min through the good Waters Sep-Pak-C of preparatory activation
18Solid phase extraction column, the pillar centrifuge dehydration of the intact back of enrichment is used the 1.0mL ethanol elution with the flow velocity of 5mL/min; The accurate adjusted volume of elutriant is to 1.0mL; With the reagent blank is reference, uses the 1cm semimicro cuvette of capacity as 0.5mL, measures absorbancy in the 610nm place.
(2) 5-p-sulfonic acid base benzeneazo-8-amidoquinaldine and the plumbous available hydrochloric acid controlling acidity that in acid medium, develops the color; The mol ratio that generates complex compound is 3: 1.The reagent maximum absorption is 420nm, and it is absorbed as 610nm with plumbous colour developing complex compound, and the system contrast gradient is very big.This coupling reaction can be at room temperature rapidly, and absorbancy can reach stable behind the placement 5min, and colour developing back system fully can be stablized 12h at least, and after SPE was with ethanol elution, color development system can be stablized 20h at least in ethanol medium.
The principle of work of analysis determining method provided by the present invention:
The available hydrophobic association principle of extraction of colour developing complex compound is explained; 5-p-sulfonic acid base benzeneazo-8-amidoquinaldine has certain hydrophobicity with the plumbous complex compound that generates, with the aqueous solution during through pillar because a little less than the elutive power of water, can not the wash-out complex compound; Therefore the complex compound that develops the color can be enriched on the pillar quantitatively; Use the strong solvent of a small amount of wash-out power (DMF, ethanol, second cyanogen, THF etc.) instead and just can get off complex compound drip washing, thus reach the colour developing complex compound enrichment.The flow velocity of pillar activation and example enrichment is 10mL/min, and pillar soaks into 2mL ethanol earlier, removes residual ethanol with the 10mL washing again; Sample (colour developing liquid) with the flow velocity of 10mL/min during through pillar complex compound and excessive reagent can be retained in fully all that (loading capacity of pillar is 50mg on the pillar; Loading capacity to complex compound is 21mg; And plumbous content only is Gamma Magnitude in the sample, therefore can not surpass the loading capacity of pillar).Promptly use the eluent wash-out after example enrichment is intact; Because ethanol is nontoxic, the weak and low price of volatility, ethanol elution is selected in this experiment for use thus, owing to just can wash the colour developing complex compound fully with the ethanol of 1mL, the enrichment multiple can reach 50 times, has improved the sensitivity of photometric analysis greatly.
Plumbous for 1.0 μ g, relative error is ± 5%, following amount ion (mg) interference measurement: K not in the sample
+, Na
+, Cl
-, Ca
2+, NH
4 +(10); PO
4 3-, Mg
2+, Al
3+, B (III), SO
4 2-, V (V) (1); Fe
3+, Co
2+, Ni
2+, Mo (VI), Zn
2+, SiO
3 2-(0.5); W (VI), Cr
3+, Ti (IV), Mn
2+, Cu
2+, Cd
2+, Sn (IV), As (V) (0.01); Pt (II), Hg
2+, Ag
+, Pd
2+(0.005) the method selectivity is better.
Compared with prior art, the present invention has following outstanding advantage:
1. institute's synthetic agent is compared with traditional 8-quinolylamine azo class reagent; Because 2 on quinoline ring is introduced methyl; Its space steric effect has stopped some interference elements and plumbous complexing beyond the deleading; The selectivity of reagent has been had significantly improve, the use of this reagent has improved the selectivity of method greatly.
2. based on new synthetic analytical reagent, set up a kind of plumbous novel method of measuring.Because method enrichment multiple reaches 50 times, the high multiple enrichment of SPE has remedied the relatively low shortcoming of absorption photometry sensitivity, makes common light-intensity method can measure the lead of μ g/g level content; Method is measured the result and is compared with graphite oven atomic absorption, and the result is consistent.
3. to have an enrichment multiple high in SPE, and environmental pollution is little, is difficult for emulsification, advantage such as save time.Described analytical reagent can generate stable violet complex with lead, and this complex compound is used spectrophotometry after with solid phase extraction concentration, and lead content and absorbance are directly proportional, and can be used for mensuration plumbous in tobacco, cigarette supplementary and the cigarette additive.
Embodiment
Through specific embodiment given below and typically used embodiment, can further be well understood to the present invention.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
Embodiment 1
---synthesizing of analytical reagent
The Sulphanilic Acid of 0.02mol is dissolved in the 400ml absolute ethyl alcohol, adds the 2g sodium amide, heating in water bath refluxed 4 hours.Add the 8g Isopentyl nitrite then, refluxed 30 minutes again, cooling makes diazonium salt.In diazonium salt solution, add the 8-amidoquinaldine of 0.02mol, 2.5g yellow soda ash stirred 0.5 hour, placed liquid, and the most ethanol of pressure reducing and steaming leaches deposition and can get bullion, and bullion promptly obtains required analytical reagent 2～3 times with ethyl alcohol recrystallization.
Embodiment 2
---the mensuration of lead in the tobacco
Accurately take by weighing tobacco 0.2g in tetrafluoroethylene microwave digestion jar, add 1.5mL concentrated nitric acid and 2mL 30%H
2O
2, in the microwave digestion stove, digest 10min; Digested back heating evaporation on hot plate and done, with the H of 20mL 5% near
2SO
4Dissolved residue changes in the 50mL tube comparison tubes; Add 5-p-sulfonic acid base benzeneazo-8-amidoquinaldine solution 4mL of 0.1% then, fully shake up, place 10min, colour developing liquid with the flow velocity of 10mL/min through the good Waters Sep-Pak-C of preparatory activation
18Solid phase extraction column, the pillar dehydration of the intact back of enrichment is used the 1.0mL ethanol elution with the flow velocity of 5mL/min, and the accurate adjusted volume of elutriant is reference to 1.0mL with the reagent blank, uses the 1cm semimicro cuvette of capacity as 0.5mL, measures absorbancy in the 610nm place.
Embodiment 3
---the mensuration of lead in the cigarette supplementary
Accurately take by weighing cigarette supplementary sample 0.2g in tetrafluoroethylene microwave digestion jar, add 1.5mL concentrated nitric acid and 2mL 30%H
2O
2, in the microwave digestion stove, digest 10min; Digested back heating evaporation on hot plate and done, with the H of 20mL 5% near
2SO
4Dissolved residue changes in the 50mL tube comparison tubes; Add 5-p-sulfonic acid base benzeneazo-8-amidoquinaldine solution 4mL of 0.1% then, fully shake up, place 10min, colour developing liquid with the flow velocity of 10mL/min through the good WatersSep-Pak-C of preparatory activation
18Solid phase extraction column, the pillar dehydration of the intact back of enrichment is used the 1.0mL ethanol elution with the flow velocity of 5mL/min, and the accurate adjusted volume of elutriant is reference to 1.0mL with the reagent blank, uses the 1cm semimicro cuvette of capacity as 0.5mL, measures absorbancy in the 610nm place.
Embodiment 4
---the mensuration of lead in the cigarette additive
Accurately take by weighing cigarette additive sample 0.2g in tetrafluoroethylene microwave digestion jar, add 1.5mL concentrated nitric acid and 2mL 30%H
2O
2, in the microwave digestion stove, digest 10min; Digested back heating evaporation on hot plate and done, with the H of 20mL 5% near
2SO
4Dissolved residue changes in the 50mL tube comparison tubes; Add 5-p-sulfonic acid base benzeneazo-8-amidoquinaldine solution 4mL of 0.1% then, fully shake up, place 10min, colour developing liquid with the flow velocity of 10mL/min through the good Waters Sep-Pak-C of preparatory activation
18Solid phase extraction column, the pillar dehydration of the intact back of enrichment is used the 1.0mL ethanol elution with the flow velocity of 5mL/min, and the accurate adjusted volume of elutriant is reference to 1.0mL with the reagent blank, uses the 1cm semimicro cuvette of capacity as 0.5mL, measures absorbancy in the 610nm place.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. the reagent that will have logical formula I is used for tobacco, cigarette supplementary or the method for measuring of cigarette additive lead content,
It is characterized in that, accurately take by weighing tobacco, cigarette supplementary or cigarette additive 0.2 g in tetrafluoroethylene microwave digestion jar, add 1.5 mL concentrated nitric acids and 2 mL, 30% H
2O
2, digestion 10 min in the microwave digestion stove; Digested back heating evaporation on hot plate and done,, changed in the 50 mL tube comparison tubess with the dissolving with hydrochloric acid residue of 20 mL 5% near; Add 5-p-sulfonic acid base benzeneazo-8-amidoquinaldine solution 4 mL of 0.1% then, fully shake up, place 10 min, colour developing liquid with the flow velocity of 10 mL/min through the good Waters Sep-Pak-C of preparatory activation
18Solid phase extraction column, the pillar centrifuge dehydration of the intact back of enrichment, with the flow velocity of 5 mL/min with 1.0 mL ethanol elutions; The accurate adjusted volume of elutriant is to 1.0 mL; With the reagent blank is reference, and the use capacity is the 1 cm semimicro cuvette of 0.5 mL, measures absorbancy in 610 nm places.
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| CN 201010256395 CN101914059B (en) | 2010-08-18 | 2010-08-18 | Analytical reagent for detecting trace lead as well as preparation method and application thereof |
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|---|---|---|---|
| CN 201010256395 CN101914059B (en) | 2010-08-18 | 2010-08-18 | Analytical reagent for detecting trace lead as well as preparation method and application thereof |
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| CN101914059A CN101914059A (en) | 2010-12-15 |
| CN101914059B true CN101914059B (en) | 2012-12-19 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507469A (en) * | 2011-10-20 | 2012-06-20 | 广东中烟工业有限责任公司 | Method for determining lead content of cigarette paper |
| CN102455293B (en) * | 2011-11-23 | 2014-07-23 | 中华人民共和国北京出入境检验检疫局 | Method for determining trace lead in textile products |
| CN103344629B (en) * | 2013-06-26 | 2016-06-29 | 天津虹炎科技有限公司 | The ICP-AES measurement method of lead content in water |
| CN103940762A (en) * | 2013-08-06 | 2014-07-23 | 江苏天瑞仪器股份有限公司 | Method for detection of lead ions in water |
| CN109557271B (en) * | 2019-01-31 | 2021-05-07 | 遵义市精科信检测有限公司 | Method and device for detecting lead metal in medicine |
-
2010
- 2010-08-18 CN CN 201010256395 patent/CN101914059B/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
|---|
| R.LONG and K.SCHOFIELD.Some Alkylquinoline-5:8-quinones.《Journal of the Chemical Society》.1953,3161-3167. * |
| 李忠,等.5-(H-酸偶氮)-8-氨基喹啉与铜显色反应研究及在烟草分析中的应用.《光谱实验室》.2000,第17卷(第6期),643-645. * |
| 胡群，等.微柱高效液相色谱法测定烟草样品中铁钴镍铜锌锰.《理化检验－化学分册》.2005,第41卷(第4期),235－237. * |
| 赵建为,等.新试剂SPAQ与铜的显色反应研究及应用.《冶金分析》.1993,第13卷(第6期),12-14. * |
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